Method and Apparatus for Obtaining Quantitative Measurements Using a Probe Based Instrument

ABSTRACT

A method includes determining the point at which a tip of a probe based instrument contacts a sample and/or the area of that contact by dynamically oscillating a cantilever of the instrument in flexural and/or torsional modes. The method additionally includes using oscillation characteristics, such as amplitude, phase, and resonant frequency, to determine the status of the contact and to provide quantitative data. Static and quasi-static measurements, including contact stiffness and elastic modulus, can be obtained from the thus obtained data. Quasistatic measurements, such as creep and viscoelastic modulus, can be obtained by repeating the static measurements for a number of force profiles at different force application rates and correlating the resultant data using known theories.

CROSS REFERENCE TO RELATED APPLICATIONS

This application is a divisional of co-pending and commonly assignedU.S. patent application Ser. No. 11/106,366; filed Apr. 14, 2005, whichclaims priority under 35 U.S.C. §119(e) to U.S. provisional ApplicationSer. No. 60/562,116, filed Apr. 14, 2004 and entitled “Method andApparatus for Obtaining Quantitative Measurements Using a Probe BasedInstrument”, the contents of which are hereby incorporated by referencein their entirety.

BACKGROUND OF THE INVENTION

1. Field of the Invention

The present invention is directed to probe-based instruments and, moreparticularly, relates to a method and apparatus for facilitating highspeed dynamic and quasi-static measurements using such an instrument. Ina particularly preferred embodiment, the invention relates to thecontrol of such an instrument to reduce or minimize lateral forces onthe probe in order, e.g., to facilitate quantitative indentationmeasurements on the nanoscale. The invention additionally relates to thetaking of indentation measurements using a probe based instrument.

2. Description of Related Art

Several probe-based instruments monitor the interaction between acantilever-based probe and a sample to obtain information concerning oneor more characteristics of the sample. For example, scanning probemicroscopes (SPMs) typically characterize the surface of a sample downto atomic dimensions by monitoring the interaction between the sampleand a tip on the cantilever probe. By providing relative scanningmovement between the tip and the sample, surface characteristic data canbe acquired over a particular region of the sample, and a correspondingmap of the sample can be generated.

The atomic force microscope (AFM) is a very popular type of SPM. Theprobe of the typical AFM includes a very small cantilever which is fixedto a support at its base and which has a sharp probe tip attached to theopposite, free end. The probe tip is brought very near to or intocontact with a surface of a sample to be examined, and the deflection ofthe cantilever in response to the probe tip's interaction with thesample is measured with an extremely sensitive deflection detector,often an optical lever system such as described in Hansma et al. U.S.Pat. No. RE 34,489, or some other deflection detector such as straingauges, capacitance sensors, etc. The probe is scanned over a surfaceusing a high-resolution three axis scanner acting on the sample supportand/or the probe. The instrument is thus capable of creating relativemotion between the probe and the sample while measuring the topography,elasticity, or some other surface property of the sample as described,e.g., in Hansma et al. U.S. Pat. No. RE 34,489; Elings et al. U.S. Pat.No. 5,226,801; and Elings et al. U.S. Pat. No. 5,412,980.

AFMs may be designed to operate in a variety of modes, including contactmode and oscillating mode. In contact mode operation, the microscopetypically scans the tip across the surface of the sample while keepingthe force of the tip on the surface of the sample generally constant.This effect is accomplished by moving either the sample or the probeassembly vertically to the surface of the sample in response to senseddeflection of the cantilever as the probe is scanned horizontally acrossthe surface. In this way, the data associated with this vertical motioncan be stored and then used to construct an image of the sample surfacecorresponding to the sample characteristic being measured, e.g., surfacetopography. Alternatively, some AFMs can at least selectively operate inan oscillation mode of operation such as TappingMode™ (TappingMode is atrademark of Veeco Instruments, Inc.) operation. In TappingMode™operation the tip is oscillated at or near a resonant frequency of thecantilever of the probe. The amplitude or phase of this oscillation iskept constant during scanning using feedback signals, which aregenerated in response to tip-sample interaction. As in contact mode,these feedback signals are then collected, stored, and used as data tocharacterize the sample.

Regardless of their mode of operation, AFMs can obtain resolution downto the atomic level on a wide variety of insulating or conductivesurfaces in air, liquid or vacuum by using piezoelectric scanners,optical lever deflection detectors, and very small cantileversfabricated using photolithographic techniques. Because of theirresolution and versatility, AFMs are important measurement devices inmany diverse fields ranging from semiconductor manufacturing tobiological research.

One potentially problematic characteristic of AFMs and other probe-basedinstruments lies in the inability to obtain some types of nanomechanicalquantitative measurements at sufficiently high speeds and/or withsufficient accuracy to meet the ever increasing demands of industry andscience.

For example, AFM's have traditionally been incapable of obtainingprecise quantitative measurement of some mechanical properties. Thisinability is increasingly problematic because the demand for suchmeasurements is rapidly increasing. For instance, polymers are beingused with increasing frequency in the semiconductor industries as “low-kdielectrics” to fill the gaps or trenches in capacitors used in memorydevices. The low-k dielectrics may have a width of 100 nanometers orless. It is often desirable to determine the mechanical properties ofthese materials.

As another example, nanophase materials such as “block copolymers”(formed from blends of two highly dissimilar polymers) are being used ina variety of applications. It is often desirable to measure thecomposition and structure of these materials on the nanometer scale.Both types of measurement require the acquisition of data obtained froman indentation measurement performed by monitoring the response of aprobe as the probe indents the sample surface. The resultant data can beused to determine elasticity modulus, plastic deformation, and othermechanical characteristics. Prior AFM's can obtain qualitativeindentation measurements using a so-called “compositional imaging”technique, but could not obtain quantified measurements.

Several hurdles prevent the transformation of traditional qualitativeinstruments into high speed and high bandwidth quantitative tools forthese nanomechanical quantitative measurements. It has been discoveredthat one of the key barriers arises from lateral forces that are appliedto the probe as result of cantilever bending. To apply a force to thesample for the purposes of, e.g., obtaining an indentation measurement,the fixed end of the cantilever is moved vertically through a distanceΔz with the tip in contact with the sample. The resultant cantileverbending generates a force k·Δz, where k is the spring constant of thecantilever. This force is not, however, applied normal to thecantilever. A component of the force instead is imposed laterally oralong the length of the cantilever. This component was historicallydeemed to be non-problematic because the lateral component of theapplied force vector is typically assumed to be much smaller than thenormal component. However, it has been discovered that the lateral forcecan in fact be an order of magnitude higher than the normal force.

The reasons for this somewhat counterintuitive characteristic of AFMoperation can be appreciated from FIG. 1, which schematically shows anAFM probe P interacting with a sample S during an indenting operation.The probe P includes a cantilever C having a tip T. The cantilever C isfixed on or formed integrally with a base B. The probe P is typicallyinclined at an angle α of about 10° to 15° relative to the surface ofthe sample S in order to assure adequate clearance between the probeholder and the sample and in order to facilitate data acquisition by aprobe detector assembly. As the probe-sample spacing in the z directionis decreased (by movement of the probe P toward the sample and/or bymovement of the sample S toward the probe P in the Z direction) toincrease the indentation force, the lateral distance available to thecantilever C in the plane L decreases. This decrease creates acompressive strain along the length of the cantilever C. Since thecantilever C has a much higher stiffness along its length in the plane Lthan perpendicular to its length in the plane N, the majority of theapplied force is actually directed in the lateral direction in the planeL.

It has also been discovered that mounting the probe P horizontally toreduce the angle α to zero does not eliminate the lateral forces on thecantilever C because of the intrinsic asymmetry of the cantilever probeconfiguration. The imposition of the unintended lateral force on thecantilever C causes a host of problems, including lateral motion of thetip T during indenting, convolution of frictional effects with elasticproperties, and non-axially symmetric application of the indentingforce.

Some current AFM indentation tools attempt to reduce the lateral forceson a probe by moving the probe laterally away from the indentation pointas the probe-sample spacing decreases. The control of this movement isopen-loop based upon historical data. It assumes the absence ofhysteresis and a constant cantilever angle. Both assumptions usuallyprove inaccurate in practice, resulting in less than optimal lateralforce counteraction.

Axially symmetric indenters have been developed. However, theseinstruments have low mechanical bandwidth (on the order of 300 Hz) andrelatively poor sensitivity because these are subject to high levels ofnoise. For instance, MTS and Hysitron produce nano-indentation devicesin which an indenter tip such as a Berkovich tip is driven into a sampleusing a multi-plate capacitor transducer system. The device has driveand pickup plates mounted on a suspension system. It provides relativemovement between the plates when the forces applied to the pickup platesdrive the probe into contact with the sample. The change in spacebetween the plates provides an accurate indication of the probesvertical movement. The input actuation forces and vertical positionreadout are therefore all-decoupled, resulting in a generally purelysymmetrical indentation process. In practice, the sensor element ismounted on a scanning tunnel microscope, and a sample is mounted on thesensor. The force sensor then can be used for both measuring the appliedforce during micro indentation or micro hardness testing and for imagingbefore and after the testing to achieve an applied AFM-type image of thesurface before and after the indentation process. Systems of this typeare described, e.g., in U.S. Pat. Nos. 5,576,483 to Bonin and 6,026,677to Bonin, both assigned to Hysitron Incorporated.

While the indenter described above provides axially symmetricindentation, it has a very low bandwidth because of the relatively largemass of the capacitive plates. The instrument also cannot obtain anaccurate image of indentations, particularly in relatively elasticsamples, because of sample rebound between the indentation and imageacquisition passes and because of the large tip radius inherent in theindenter tip. It also has relatively poor force sensitivity, on theorder of 15 nano-Newtons, as opposed to a few pico-Newtons for a trueAFM having a much smaller tip.

Other obstacles have also heretofore prevented AFM-based quantitativeindentation measurements.

For instance, prior AFM-based indenters, like other indenters, indentedthe sample and acquired indentation data in two separate steps. That is,the sample is first indented using a probe to create an indent. Then,after the probe is removed from the indent, a raster scan or similarscanning technique is used to image the indent. However, the acquiredimage does not accurately reflect the indent for at least two reasons.First, the tip cannot accurately reflect deformation geometry. Second,an elastic material will at least partially recover or “rebound” betweenthe indentation and imaging passes, resulting in partial disappearanceof the indentation. In the worst case scenario of a near perfectlyelastic sample surface, the indentation will nearly completely disappearbetween the indentation and imaging passes.

For instance, the displacement of a material in response to a given loadprovides useful information regarding property characteristics,including elastic modulus E_(sample) and the plastic deformation. Loadsare typically imposed by indenting a sample surface with a probe andmeasuring properties of the resulting indentation. The sample isindented through an indentation cycle having a “loading phase” in whichthe tip is driven into and indents the sample surface and a subsequent“unloading phase” in which the tip is withdrawn from the sample surface.

The load-displacement relationship resulting from an indentation cycleis expressed in the form of Hook's law for indentation induceddeformations. Hook's law, which expresses the relationship between forceand deformation, is expressed as follows:

L=a(h _(max) −h _(f))^(m)  (1)

where:

-   -   L is the load applied to the cantilever probe,    -   h_(max), or penetration depth, represents maximum tip        penetration into the sample during the indentation cycle; and    -   h_(f), or plastic indentation depth, is the plastically deformed        part of the penetration depth h_(max) which does not recover        after load withdrawal.

During a typical indentation cycle, the loading probe will indent thesample to h_(max) at the end of the loading phase when the applied loadis the highest. Then, during the unloading phase, the unloading probewill separate from the bottom of the indentation at a release pointP_(r) above the point P_(max) located at the lower limit of h_(max). Thederivative of equation (1) is called contact stiffness, S. S at anygiven depth h during deformation can be expressed as:

$\begin{matrix}{S = \frac{L}{h}} & (2)\end{matrix}$

The static contact stiffness for an entire indentation cycle can beexpressed as:

$\begin{matrix}{S = \frac{\Delta \; L}{\Delta \; h}} & (3)\end{matrix}$

If lateral forces on the tip are counterbalanced, ΔL can be easilydetermined simply by detecting the vertical load, L_(max), at the end ofthe loading phase of the indentation cycle. Δh can be determined bysubtracting the maximum penetration point P_(max) from the initialcontact point, P_(ic), where the probe first engages the sample surface.P_(max) can be measured directly using conventional monitoringtechniques. P_(ic) measurements are more difficult, and are part of apreferred embodiment of the invention.

S is dependent upon material properties as follows:

$\begin{matrix}{S = {\frac{2}{\sqrt{\pi}}E_{r}\sqrt{A_{con}}}} & (4)\end{matrix}$

where

-   -   E_(r) is the reduced modulus of the sample/tip interaction; and    -   A_(con) is the contact area during deformation, which is a        function of indentation depth h;

The relationship between the elastic modulus of the E_(sample) and E_(r)can be expressed as follows:

$\begin{matrix}{\frac{1}{E_{r}} = {\frac{( {1 - v_{sample}^{2}} )}{E_{sample}} + \frac{( {1 - v_{tip}^{2}} )}{E_{tip}}}} & (5)\end{matrix}$

where:

-   -   E_(tip) is the elastic modulus for the tip, which is known for a        tip of a known material, and    -   V_(sample) and V_(tip) are the Poisson ratio for the sample and        the tip, respectively.

Poisson ratios vary only minutely from material to material, soV_(sample) can be assumed to be close to V_(tip), which is a knownconstant C for a known tip material. Hence, equation 5 can, as apractical matter, be reduced to:

$\begin{matrix}{\frac{1}{E_{r}} = {\frac{( {1 - c^{2}} )}{E_{sample}} + \frac{( {1 - c^{2}} )}{E_{tip}}}} & (6)\end{matrix}$

Referring again to Equation (4), E_(r) can be determined from a measuredcontact area A_(con) using the equation:

$\begin{matrix}{E_{r} = {\frac{\sqrt{\pi}}{2\sqrt{A_{con}}}s}} & (7)\end{matrix}$

Hence combining equations (6) and (7), the sample elastic modulusE_(sample) can be determined as follows:

$\begin{matrix}{E_{sample} = {( {1 - c^{2}} )/( {( {2{\sqrt{A_{com}}/\sqrt{ \pi )}}} ) - \frac{( {1 - c^{2}} )}{E_{tip}}} )}} & (8)\end{matrix}$

Practically speaking, the greatest challenge for quantitative mechanicalmeasurements is to measure the contact area, A_(con), which is afunction of the actual contact depth, h_(cact), and the tip shape. Theactual contact depth usually is not the same as the penetration depth,h_(max), because a sample having any elasticity will deform away fromthe tip at the upper portion of the indentation, leaving a space, h_(s),between the upper limit of the h_(cact) and the initial contact pointP_(ic), as can be appreciated from FIG. 13A. The possible variations inthis discrepancy can be appreciated from a comparison of FIG. 14A andFIG. 14B, which illustrate the indentation of the same tip T into thehighly plastic sample S₁ and a highly elastic sample S₂, respectively.In a plastic sample, the material conforms closely to the shape of thetip T throughout the depth of the indent I, the contact area and indentarea are essentially the same. In contrast, in a highly elastic sample,only a small portion of the tip above the apex A is embedded in thesample at the bottom of the indentation stroke. The remainder of theembedded portion of the tip T is surrounded by a free space extendingradially from the tip T to the perimeter of the indent I, resulting inan indent area that is much larger than the area of the imbedded portionof the tip.

In addition, the lower limit of h_(cact), being the point of separationof the apex of the tip from the bottom of indentation during theunloading phase of the indentation cycle (hereafter referred to as the“release point”, P_(r)), is not the same as the deepest penetrationpoint P_(max). This is because a sample having any significantelasticity will rebound as the tip is being withdrawn from the sample,resulting in a P_(r) that is above P_(max) as seen in FIG. 13B. As aresult, the actual contact depth h_(cact) required for elastic modulusdetermination is reduced by the difference between P_(max) and P_(r).

A determination of h_(cact) therefore requires a determination of thelocation of both the release point P_(r) where the apex of unloading tipfirst separates from the bottom of the rebounding indent, and the upperseparation point, P_(sep), where no portion of the unloading tipcontacts the detent.

The initial contact point, P_(ic), is often determined simply bydetermining the location at which the force imposed on the loadingcantilever markedly changes during the loading phase of the indentationcycle. Referring to the force displacement curves 15 and 18 of FIG. 15,that point is relatively accurately determinable for a relatively hardsurface which has a marked reaction to initial contact, evidenced by a“snap to contact” as a result of adhesive forces arising when the probecomes into close proximity with the sample surface, followed by a sharpincrease in force as the probe is driven against the sample surface.That resistance is evidenced by the steep slope of the curve 15 afterthe initial “snap to contact” at point 16 in FIG. 15. However, in thecase of a relatively soft sample such as a gel, the sample surfaceprovides very little initial resistance to tip motion after the tipcontacts the surface. The tip may drive well into the sample surfacebefore the threshold resistance allegedly indicative of contact point isreached, resulting in an inaccurate determination of initial contactpoint. This problem can be appreciated by the very shallow andill-defined slope of the curve 18 in FIG. 15.

A need therefore exists for a more accurate detection of initial contactpoint P_(ic), particularly in the case of indenting relatively softsamples.

Prior systems also have difficulty determining the release point, P_(r),and the actual contact depth, h_(cact) during indentation becausematerial measurements are taken in a separate scanning operationsometime after the tip is removed from the indented sample. If thesample is relatively elastic or viscoelastic, creep, defined as changesin elastic deformation over time, will alter both the depth and area ofthe indent as the sample rebounds toward its original shape followinginitial tip removal.

In summary a quantitative mechanical property determination withcantilever probe based AFM the following aspects should be adequatelyaddressed:

1. The load must be well defined. Since the cantilever sensor isprimarily a flexural sensor, the lateral force along the cantilever axisis unknown and should be counteracted prior to determining load.

2. Contact points, including initial contact point, P_(ic), the releasepoint, P_(r), and the separation point, P_(sep), should be accuratelymeasured.

3. With the knowledge of the tip shape, the contact area can bedetermined quantitatively.

Furthermore, the need has broadly arisen to provide a probe basedinstrument that is capable of obtaining high speed, high bandwidthquantitative measurement of mechanical properties through indentationand other interactions. It is believed that in order to meet theseneeds, the lateral component of AFM based indentation needs to bereduced by 2 to 3 orders of magnitude than is usually achievable usingcurrent techniques.

Partially in order to meet the above-identified need, and partially inorder to achieve other benefits like more controlled tip-sampleinteraction, the need has also arisen to effectively and reliablycounteract the lateral forces imposed on a probe as a result ofprobe-sample interaction.

SUMMARY OF THE INVENTION

In accordance with one aspect of the invention, a method includesdetermining the point at which a tip of a probe based instrumentcontacts a sample and/or the area of that contact by dynamicallyoscillating a cantilever of the instrument in flexural and/or torsionalmodes. The method additionally includes using oscillationcharacteristics, such as amplitude, phase, and resonant frequency, todetermine the status of the contact and to provide quantitative data.Static and quasi-static measurements, including contact stiffness andelastic modulus, can be obtained from the thus obtained data.Quasistatic measurements, such as creep and viscoelastic modulus, can beobtained by repeating the static measurements for a number of forceprofiles at different force application rates and correlating theresultant data using known theories (see A. S. Nowick and B. S. Berry,Anelastic Relaxation in Crystalline Solids, Academy Press, 1972).

Initial contact point P_(c) can be unambiguously determined bymonitoring operation of an oscillating probe because, at the onset ofeven an extremely small contact force occurring at the beginning of theprobe's loading phase of an indentation cycle, measurable change in theresonant properties will be evident, providing a precise indication ofinitial contact point. Preferably, the probe is driven in so-called“torsional resonance” mode, whereby the cantilever is excited toresonate in torsion and the AFM detects changes in amplitude, phase, orfrequency in response to surface interactions. (See U.S. Ser. Nos.10/189,108 and 10/937,597, each of which is expressly incorporated byreference herein) The motion of the apex of the probe's tip in this modeis typically less than a nanometer, but the torsional resonance has aparticularly strong dependence on the frequency, amplitude, and phasechanges with tip sample separation.

The actual contact depth h_(cact) can similarly be measured bymonitoring interaction between an unloading cantilever and the samplewhile imparting oscillating relative movement between the probe and thesample. For instance, when torsional resonance is superimposed on anunloading cantilever, a torsional resonant amplitude could develop assoon as the tip has an angstrom-range length of space to oscillatewithin the indentation, occurring at the release point, P_(r). As thetip continues to unload, the average space between the tip and theperimeter of the indentation increases with a resultant change intorsional amplitude or phase. The separation point, P_(sep), can bedetected when the monitored tip oscillation characteristic approachesoscillation in free air, indicating that no portion of the oscillatingprobe is engaging the indentation perimeter. The actual contact depthh_(cact) can be determined by subtracting the detected separation point,P_(sep), from the detected release point, P_(r). Penetration depthh_(max) can be determined by subtracting the determined initial contactpoint P_(ic) from a directly detected probe position at the maximumpenetration depth h_(max). Contact area A_(con) can also be determinedfrom the data acquired during the unloading phase of the indentationcycle, provided that the tip is “characterized” i.e., provided that thesize and shape of the tip are known so that the surface area of the tipis known. Tip characterization may be achieved, e.g., by directmeasurement, and/or by using a reconstruction algorithm that employs acharacterizer with a precisely known shape.

These and other features and advantages of the invention will becomeapparent to those skilled in the art from the following detaileddescription and the accompanying drawings. It should be understood,however, that the detailed description and specific examples, whileindicating preferred embodiments of the present invention, are given byway of illustration and not of limitation. Many changes andmodifications may be made within the scope of the present inventionwithout departing from the spirit thereof, and the invention includesall such modifications.

BRIEF DESCRIPTION OF THE DRAWINGS

A preferred exemplary embodiment of the invention is illustrated in theaccompanying drawings in which like reference numerals represent likeparts throughout, and in which:

FIG. 1 schematically illustrates operation of a conventional passiveprobe of an AFM during a sample indentation process, appropriatelylabeled PRIOR ART;

FIG. 2 schematically illustrates operation of a conventional activeprobe of an AFM during a sample indentation process; appropriatelylabeled PRIOR ART;

FIG. 3 schematically illustrates a prior art technique for obtainingindentation measurements using an AFM, appropriately labeled PRIOR ART;

FIGS. 4 a-4 c are finite element analysis diagrams simulating operationof various prior art probes during sample indentation processes,appropriately labeled PRIOR ART;

FIGS. 5 a-5 b are finite element analysis diagrams simulating operationof inventive probes during a sample indentation process;

FIG. 6A schematically illustrates an AFM constructed in accordance witha first preferred embodiment of the present invention;

FIG. 6B schematically illustrates an AFM constructed in accordance witha second preferred embodiment of the present invention;

FIG. 7A is a flowchart of a process usable to control the AFM of FIG. 6Aor 6B to obtain indentation measurements while counteracting lateralloads on the AFM's probe;

FIG. 7B is a flowchart of an alternative process usable to control theAFM of FIG. 6A or 6B to obtain indentation measurements whilecounteracting lateral loads on the AFM's probe;

FIG. 8A schematically illustrates the contacting of a sample surfacewith a probe tip during relative oscillation of the probe and/or thesample in the X-Y plane;

FIG. 8B is a graph illustrating a phase shift occurring upon the initialcontact illustrated in FIG. 8A;

FIGS. 9A-9D collectively schematically illustrate a technique forobtaining indentation measurements on a real time basis, with FIGS.10A-10D illustrating the resonances experienced by the probe at eachstage of the measurement illustrated in FIGS. 9A-9D, respectively;

FIGS. 11A-11D are a series of graphs illustrating the full range ofcantilever response during the loading phase of an indentation cycle;

FIG. 12 is a flowchart for obtaining material property measurements inaccordance with a preferred embodiment of the invention;

FIGS. 13A and 13B schematically illustrate the indentation of an elasticor visco-elastic sample using a probe tip;

FIG. 14A schematically illustrates the indentation of a highly plasticsample with a tip;

FIG. 14B schematically illustrates the indentation of a highly elasticsample with a tip; and

FIG. 15 is a graph illustrating AFM force curves for both hard and softsamples.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS 1. Lateral ForceCounteraction

One AFM described herein uses controlled actuation of an “activecantilever” to reduce or eliminate lateral forces on a probe of an AFMor other probe-based instrument when taking mechanical measurements,hence permitting the formation of axially symmetric indents and theaccurate determination of applied vertical load. Because the loads aremost problematic when taking indentation measurements, an embodimentwill now be described in conjunction with an AFM configured to functionas an indentation measuring tool. However, the lateral force reductiontechniques discussed herein are usable during other measurements and onother instruments as well.

In the presently preferred embodiment, the indentation force is appliedthrough a combination of a conventional z-actuator and an “activecantilever.” The active cantilever could be any number of cantileversthat can be deformed in a controlled manner. It may, for example, be onethat deforms under induced thermal stress, one that deforms underelectromagnetic forces, one that deforms under ultrasonic pressure,and/or one that deforms under photon pressure. It preferably ispiezoelectric composite cantilever, more preferably one that contains alayer of a ZnO piezoelectric film, for instance, between two metalelectrodes deposited on a silicon cantilever, thus forming a “bimorph”device. By applying a voltage to the actuator's electrodes, the actuatorbends towards or away from the sample surface. Active cantilevers ofthis type were originally developed for AFMs at Stanford University.Similarly, active cantilevers and control systems are described, forinstance, in U.S. Pat. No. 5,317,533 to Quate et al. and U.S. Pat. Nos.6,672,144 and 6,189,374 to Adderton et al., the disclosures of each ofwhich are hereby incorporated by reference in their entirety.

It has been discovered that an active cantilever on a z positionactuator can be controlled to balance the lateral loads imposed on theprobe during an indenting operation. Referring again to FIG. 1, aconventional passive cantilever C applies a force F on the sample Shaving a lateral component that extends away from the laterally fixedprobe base B. Conversely, as can be appreciated from FIG. 2, a probe P1having a self-actuated bimorph cantilever C1 applies a force F1 having alateral component that extends toward the laterally fixed probe base B.Because the lateral forces due to passive cantilever motion and activecantilever voltage loading are of the opposite signs, the two forceapplication methods can be used to balance the lateral loads, providedthat they are used simultaneously and properly scaled. This effect isdemonstrated schematically in FIG. 3, in which the tip T2 of an activecantilever C2 of a probe P2 indents a sample S. As the probe-samplespacing z decreases, the active cantilever C2 can be actuated to cancelthe lateral component of the force imposed by passive movement,resulting in the imposition of a purely normal force F2 on thecantilever C2 and a purely vertical force on the sample (provided thatthe tip T2 is mounted at an angle that compensates for the incline ofthen cantilever C2).

Finite element analysis simulations demonstrate the possibility ofgenerating purely vertical forces through lateral force cancellation.FIGS. 4 a-5 b illustrate force plots during indentation using acantilever that is moved 100 nm into contact with a sample, thecantilever being 100 μm long by 8 μm thick. FIGS. 4 a-4 c plot the datafor an inclined passive probe configured as discussed above in FIG. 1,an inclined active probe configured as discussed above in conjunctionwith FIG. 2, and a horizontal passive probe, respectively. All threesimulations confirm that substantial lateral forces are generated duringthe indentation process—forces that are about twice the vertical forcesin the case of the commonly employed inclined passive probe. Acomparison of FIGS. 4 a to FIG. 4 b also confirms that the lateral forcecomponents are in opposite directions for active and passive probes.Conversely, FIG. 5A confirms that coordinating control of an activecantilever and a z position actuator can balance the lateral forces onan inclined cantilever, resulting in the imposition of purely verticalforces on a sample. FIG. 5 b similarly confirms that coordinatingcontrol of an active cantilever and a z position actuator can balancethe lateral forces on a horizontal cantilever resulting in theimposition of purely vertical forces on a sample. The data illustratedgraphically in FIGS. 4 a-5 b is confirmed numerically in Table 1:

TABLE 1 Forces Generated During Indentation Vertical Force Lateral ForceTotal Force Case (nN) (nN) (nN) 1 (FIG. 4a) 825 −1200.0 1456 2 (FIG. 4b)769 570 957 3 (FIG. 4c) 426 206 474 4 (FIG. 5a) 774 0 774 5 (FIG. 5b)706 0 706

The lateral forces could be canceled through open loop control of theactive cantilever based on known cantilever properties. It is currentlypreferred, however, to use closed loop control to counteract theunwanted lateral forces. The currently preferred embodiment applies avoltage to at least one of (1) the piezoelectric bimorph of the activecantilever and (2) a separate z position actuator and adjusts thez-piezo voltage according to the variation of cantilever deflection tomaintain the angle α of the free end of the cantilever C2 (FIG. 3)constant. The voltage applied to the piezoelectric bimorph 36 of theactive cantilever therefore represents the applied force, and thedisplacement of the z-actuator represents the apparent penetration depthat any given time. (It is still necessary to adjust the apparentpenetration depth by the “frame compliance,” to obtain the truepenetration depth h_(max). This correction is a commonly used techniquein indentation experiments.) Two AFMs configured to achieve this effectand a method of achieving it will now be described.

Referring now to FIG. 6A, an AFM 10 constructed in accordance with afirst embodiment of the present invention is shown that has a probeassembly 18 configured to indent a sample S mounted on a support (notshown) which may be either fixed our movable. The probe assembly 18 ofthis embodiment is mounted on the bottom of a z position actuator 16 soas to be movable in a z direction which is perpendicular to an xy planeof the sample support. The z direction is typically vertical. Probeassembly 18 includes a self-actuated cantilever 20 having a tip 26 thatinteracts with a sample S during indentation. Cantilever 20 includes afixed end 22, preferably mounted to an AFM mount (not shown) and a free,distal end 24 that receives tip 26. Cantilever 20 also bears apiezoelectric bimorph element 36 that can be energized to bend thecantilever 20 and, hence, raise and lower the tip 26. In operation, theinteraction between tip 26 and sample surface 28 deflects the cantilever20. To measure this deflection, AFM 10 includes a deflection detector 30that may preferably be an optical detection system for measuring thecantilever deflection by any suitable method. Suitable methods include:

-   -   an optical beam bounce technique (see, e.g., Meyer and Amer,        “Novel Optical Approach to Atomic Force Microscopy,” Appl. Phys.        Lett. 53, 1045 (1988); Alexander, Hellemans, Marti, Schneir,        Elings, Hansma, Longmire, and Gurley, “An Atomic-Resolution        Atomic-Force Microscope Implemented Using an Optical Lever,”        Appl. Phys. Lett. 65 164 (1989)); or    -   an interdigital diffraction grating technique (Manalis, Minne,        Atalar, and Quate, “Interdigital Cantilevers for Atomic Force        Microscopy,” Appl. Phys. Lett., 69 (25) 3944-6 (1996);        Yoralioglu, Atalar, Manalis, and Quate, “Analysis and design of        an interdigital cantilever as a displacement sensor,” 83(12)        7405 (June 1998)); or    -   any other known optical detection method.

As is typical, the optical-based deflection detector 30 includes a laser50 and a photodetector 52 that interact according to one of the abovetechniques. The resultant data produce information reflecting verticaland lateral deflection of the cantilever. That information can then bedemodulated, either in external analogue or digital circuitry locatedexternal to the controller 34 (detailed below), or circuitry within thecontroller, to obtain information regarding the lateral and verticalpositions of the probe, as well as phase information, if the probe 18 isoperating in an oscillating mode such as TappingMode operation. Whenused in conjunction with very small microfabricated cantilevers andpiezoelectric positioners as lateral and vertical scanners, AFMs of thetype contemplated by the present invention can have resolution down tothe molecular level, and can operate with controllable forces smallenough to image biological substances.

With further reference to FIG. 6A, AFM 10 operates to precisely indentthe sample S while maintaining the angle of the free end 24 of thecantilever 20 constant. In particular, instrument 10 includes acontroller 34 that subtracts the setpoint SP from the cantileverdeflection signal Ds, thereby generating an error signal that is atleast indirectly indicative of a change in cantilever free end angle.Controller 34 is preferably a PI or PID controller. Controller 34 can beimplemented in either analog or digital, and may apply either a lineargain or a gain characterized by a more complex computation. Inparticular, controller 34 can apply a gain to the error signal that isdefined by one or more of a proportional, an integral or a differentialgain.

Controller 34, in response to the error signal, generates a controlsignal using a feedback controller 35 and transmits the control signalto the piezoelectric z-actuator 16 in order to maintain the angle α ofthe free end 24 end of the cantilever 20 constant. However, z-piezoactuators are typically nonlinear and have substantial hysteresis. Inorder to make a precise measurement of vertical position, as is requiredfor quantitative indentation, an independent z-sensor 40 is preferablyemployed to monitor operation of the z position actuator 16 underfeedback. In the preferred embodiment, the sensor 40 is one recentlydeveloped by Veeco Instruments that provides an RMS noise floor of <0.05nm in a 1 kHz bandwidth with a maximum range of 10 μm.

The controller 34 or a separate dedicated controller (not shown) alsouses a feedback controller 37 to energize the bimorph element 36 underfrom the detector 52 to move the probe 18 in the z direction to indentthe sample. Indentation is controlled under feedback from the deflectiondetector 34. Because, the lateral forces imposed on the cantilever 20remain counteracted during indentation due to the simultaneous controlof the z-actuator 16 as discussed above, the force on the sampletherefore is a simple function of the indentation feedback voltageapplied to the piezoelectric bimorph 36 of the active cantilever 22. Ifthe frame compliance is neglected, the applied force is F=k·S·V, where Fis the applied force, k is the cantilever spring constant, S is thepiezobimorph sensitivity, and V is the applied voltage.

The controller 34 can determine the initial contact point P_(ic), therelease point P_(r), the separation point P_(sep), the actual contactdepth h_(cact), and contact area A_(con) from the resultant informationas described in greater detail below. Those parameters, in turn, can beused to determine sample properties of interest such as contactstiffness and, plastic deformation, and elastic modulus in a mannerwhich is, per se, well known. These and other properties can then bemanipulated further and/or displayed in a display device (not shown)such as a monitor.

It should be noted that, instead of using the bimorph element 36 forindentation control and the z position actuator 16 for lateral forcecounter feedback control, the roles of these two actuators could bereversed. In that case, the z position actuator 16 will be controlled tomaintain the cantilever in a commanded position under feedback, and thebimorph element 36 will be controlled to counteract lateral forces inthe cantilever. In addition, it should be understood that the z positionactuator 16 could be used to move the sample S rather than the probe 18.

A more sophisticated AFM configured to counteract lateral forces on theprobe during indentation is illustrated in FIG. 6B. The AFM 110 of thisembodiment is similar to the AFM of the embodiment of FIG. 6A, andcomponents thereof having corresponding components to those of FIG. 6Aare therefore designated by the same reference numeral, incremented by100. The AFM 110 therefore includes a z position actuator 116 and apiezoelectric bimorph element 136 mounted on a cantilever 120. The AFM110 also includes a deflection detector 130 that preferably includes alaser 150 and a photo detector 152. It also includes a controller 134and a z position sensor 140.

The AFM 110 of this embodiment differs from the AFM of the firstembodiment in that it includes an additional XY actuator 112 which canbe energized to permit counteraction of forces in the XY plane in orderto prevent any movement of the tip in the Y direction or into and out ofthe page in the drawings. That is, digital or analog circuitry 154 canrely on signals from the detector 150 to determine lateral deflection inthe Y direction, and those signals can be compared to a set point of afirst feedback controller 135 of the controller 134 to move the XYactuator 112 to prevent movement of the tip in the Y direction duringindentation, preferably by keeping a rotational angle of the cantileverfree end constant. The same XY actuator 112 can be controlled underfeedback to position the probe 118 over the sample S at a desiredlocation for indentation and image acquisition. As with the previousembodiment, a feedback controller 135′ within the controller 134 alsotransmits a control signal to the z actuator 116 under feedback from thedetector 152 to maintain the angle of the end of cantilever 120constant, while an additional controller 137 is activated under feedbackto indent the sample S under feedback. Also as in the previousembodiment, it should be understood that one or both of the actuators112 and 116 could be used to move the sample S rather than the probe118.

Referring to FIG. 7A, a possible process 200 for controlling the AFM 10of FIG. 6A or the AFM 110 of FIG. 6B to obtain indentation measurementssuch as force curves and/or elasticity measurements while counteractinglateral forces includes two loops: one Loop 202 that maintains thecantilever deflection constant, and another Loop 204 that adjusts activelever voltage and measures z-sensor voltage to obtain indentationmeasurements. The Loops 202 and 204 can run synchronously and integratedor entirely asynchronously.

During the indentation process, Loop 202 proceeds from START in Block206 to Block 208 to measure the position of a portion of the probeassembly, preferably the deflection of the cantilever's free end. Loop202 then proceeds to Block 210, where the cantilever deflection iscompared with a desired setpoint, and an error signal is generated thatpreferably is proportional to the difference between the detecteddeflection and the setpoint deflection. Again, this deflection isindicative of cantilever free end angle, but need not be a directmeasurement of the angle. Loop 202 then proceeds to Block 212, where thecontroller causes a voltage to be delivered to the XY actuator and/orthe z actuator to minimize or null the error signal, hence maintainingthe cantilever deflection constant despite changes in probe-samplespacing and tip depth penetration during the indenting process. Thelateral forces on the cantilever 20 therefore are counteracted. Loop 202then returns to Block 208, where the operations of Blocks 200 and 202are repeated on a continuous basis.

Loop 204 also proceeds from START 206 and then proceeds to Block 214,where voltage is applied to the cantilever's piezoelectric element tomove the probe toward the sample and generate a force on the sample toultimately generate a commanded force profile F(t). Due to thecounteraction of lateral forces on the probe using the Loop 202, theforce imposed on the sample is a simple function of the known voltageapplied to the piezoelectric bimorph element. The Loop 204 then proceedsto Block 216, where the z position of the probe assembly is determinedusing the z-position sensor, hence providing the z position informationrequired to obtain force vs. position data for that point on theprofile. The Loop 204 then checks in Block 218 to determine whether theprofiling process is complete, and, if not, cycles through Blocks 214,216, and 218 until the profile is complete. The resultant data can beused as generally denoted by Block 220, e.g., to determine any of anumber of sample characteristics, some of which are discussed below.This information can be displayed directly and/or combined with otherproperties of the sample to determine other sample properties. The probeassembly is then moved away from the sample and, if desired,repositioned over another point on the sample surface, where the process200 is repeated.

A more generalized alternative process 230 for controlling either theAFM 10 of FIG. 6A or the AFM 110 of FIG. 6B is illustrated in FIG. 7B.As a practical matter, the process 230 differs from the process 200discussed above in connection with FIG. 7A only in that the activecantilever is used for indentation and at least the z position actuator,and possibly the xy actuator (if present), are controlled to maintainthe cantilever free end deflection angle constant. Hence, the process230 first proceeds from Start in Block 232 to cause the probe tointeract with the sample in Block 234. An indentation loop 236 is thenimplemented in which the active cantilever is energized to indent thesample surface in Block 240 to perform an indentation cycle as generallyreferenced in Block 242 using the technique discussed above.Simultaneously, a lateral force counteraction loop 238 is implementedvia which cantilever free end deflection is measured in Block 244, anerror signal is generated in Block 246, and the appropriate z positionand/or xy position actuator(s) are controlled under feedback in Block248 to maintain the cantilever deflection angle constant despite changesin probe/sample spacing and probe penetration depth.

As with the process 200, after the indentation cycle is complete, theprocesses of loops 236 and 238 can be repeated as many times as isneeded to generate a force profile (see inquiry Block 250) useful forquasistatic measurements such as creep and viscoelastic modulus,whereupon the process 230 proceeds to End in Block 252.

2. Quantified Material Property Measurements

As discussed above, dynamic and quasistatic measurements can be combinedto unambiguously determine the initial contact point P_(ic), actualcontact depth h_(cact), and other parameters of the indentation. Thesemeasurements are taken during the “loading phase” of the indentationcycle in which the tip is driven into and indents the sample surface andthe subsequent “unloading phase” in which the tip is withdrawn from thesample surface. The preferred technique involves monitoring proberesponse while imparting oscillating movement between the tip and thesample during the loading phase of the indentation cycle to determinethe initial contact point P_(ic) and during the unloading phase todetermine actual contact depth h_(cact).

Particularly during the loading phase, the relative movement could be arelative vertical movement caused, e.g., by exciting the probe tooscillate about the z-axis in flexural resonance. The initial contactpoint P_(ic) is then detected by detecting a change in probe operationoccurring as a result of tip-sample interaction occurring at the contactpoint. A possible operational mode is TappingMode, in which the probe isdriven to oscillate at or near its resonance flexural frequency whilethe probe/sample spacing is decreased under feedback and a change inprobe oscillation amplitude and/or frequency indicative of samplecontact is detected.

It is currently preferred, however, that relative lateral oscillatingmovement be used as a source of both contact point detection and contactdepth detection. Relative lateral movement could be made by shaking thesample and/or the probe as a whole along one or both axes of the XYplane in a manner that is, per se, well known. The preferred technique,however, utilizes torsional resonance or TR-Mode™ mode, which wasrecently commercialized by Veeco Instruments, Inc. In TR-Mode, acantilever is excited to resonate at a torsional resonance, and a changein amplitude, phase or frequency in response to surface interactions isdetected. (Torsional resonance imaging is discussed, for example, inU.S. patent application Ser. Nos. 10/189,108 and 10/937,597 filed Jul.2, 2002 and Sep. 9, 2004, respectively, the subject matter of which ishereby incorporated by resonance in its entirety). The motion of theapex A of the tip T in TR mode is typically less than 1 nm, but thetorsional resonance has a particularly strong dependence on thefrequency, amplitude, and phase changes with tip-sample separation,permitting extremely precise detection of initial tip/sample interactionduring the loading phase and initial separation during the unloadingphase. The Q of TR mode is also very high, typically 1,000 to 2,000. Asa result, the tip-sample interaction force, which is inverselyproportional Q, does not deter the unloading deformation process in thevertical z direction. Both initial contact point determination andactual contact depth determination will now be described in greaterdetail.

As seen in FIGS. 8A and 8B, a tip T resonating in free space has a freespace resonance peak or simply “free air peak” f₀ at a particularfrequency. As soon as the apex A of the tip T contacts the samplesurface S, the mechanical boundary of the oscillation changes, resultingin the generation of a contact resonant frequency peak or simply“contact peak” f_(c) at a different frequency than the free air peak f₀.The initial contact point P_(ic) can be unambiguously determined bynoting the onset of the contact peak f_(c). As is to be expected, theamplitudes of the two peaks f₀ and f_(c) are inversely are related sothat f_(c) is zero and f₀ is maximized when the cantilever oscillates infree air and f_(c) is maximized and f₀ is minimized when the tip T isfully indented into the sample surface S at the end of the loadingphase.

Penetration depth P_(max), can be determined by monitoring the positionof the probe at the juncture between the loading and unloading phase,taking frame compliance into account in a known manner. The maximumapplied force can also be measured in a conventional manner at thistime, hence permitting determinations of ΔP and Δh for contact stiffnessdetermination.

Determining onset of the contact peak f_(c) during tip withdrawalprovides an indication of the release point, P_(r), and, accordingly, abottom limit of the actual contact depth, h_(act), and determining theduration of the contact peak f_(c) provides an indication of contactarea.

This effect is illustrated schematically in FIGS. 10A-10B, whichillustrate the frequency resonance of a tip T during part of theindentation cycle illustrated in FIGS. 9A-9D. Oscillation preferably ismodulated at a much higher frequency and lower amplitude during theunloading stage to explore the free space surrounding the tip. In TRmode, the tip T is preferably oscillated in the megahertz range duringunloading and the kilohertz range during loading. In FIG. 9A, the tip Thas not yet come into contact with the sample S, resulting in a free airpeak f₀ of a maximum value and no contact peak f_(c) as seen in FIG.10A. Conversely, at the end of the loading phase of the indentationcycle in which the tip T is fully imbedded in the indent I as seen inFIG. 9B, the free air peak f₀ is a zero and the contact peak f_(c) is ata maximum as seen in FIG. 10B. During the subsequent unloading phase ofthe indenting cycle, the contact peak f_(c) of the unloading tip T willdevelop as soon as the apex A of tip has an angstrom-range room tooscillate, i.e., immediately after the apex A of the unloading tipleaves the bottom of the indent I. The detection of the resultant changein oscillation amplitude and/or frequency, coupled with a preciseknowledge of probe position using the indenting feedback controltechnique discussed above, provides a very accurate determination therelease point, P_(r), or the bottom of the indent.

Contact resonance evolution as the tip moves towards and indents thesample during progressive zones of the loading phase of the indentationprocess is illustrated by FIGS. 11A-11D. In the initial or free zone ofthe loading phase in which the tip has not yet engaged the samplesurface, the cantilever oscillates freely at a first frequency and arelatively high amplitude as can be seen at point F on the curve 260 ofFIG. 11A and the curve F of FIG. 11B. When the tip engages the surface,the free resonance diminishes and the contact resonance starts todevelop, as indicated by the point O at the intersections of curves 260and 262 in FIG. 11A and the existence of both curves in FIG. 11C. As theloading phase proceeds (shown as A, B, C on curve 262 in FIG. 11A, withthe resonance curve development shown in FIG. 11D) the amplitude of thecontact resonance will continue to grow for a time and then diminish,while the resonance frequency shifts throughout the indentation phasedue to the increase of the contact stiffness. A comparison of thecontact resonance curve 262 at points O, A, B, and C to the point F onfree resonance curve 260 in FIG. 11A shows that the contact resonanceamplitude throughout the indentation phase is less than the freeamplitude prior to probe/sample contact.

FIGS. 11A-11D only show one of the many contact modes developed duringindentation contact depths change. Other modes includes, but are notlimited to, torsional contact resonances of different modes, flexuralcontact resonances of different modes, and sub-resonance oscillation atdifferent frequency.

As the tip is withdrawn from the sample as seen in FIG. 9C, both contactresonance oscillation and free air resonance oscillation are detectableas seen in FIG. 10C, with the magnitude f₀ progressively decreasing andthe magnitude of f_(c) progressively increasing. Some f_(c) componentswill remain so long as any portion of the oscillating tip contacts thesample. The contact peak f_(c) will disappear only when no portion ofthe tip interacts with the sample, which occurs at the separation pointP_(sep) of the tip withdrawal process. The actual contact depth h_(cact)can now be determined simply by subtracting P_(sep) from P_(r). Contactarea A_(con) can be determined from the actual contact depth h_(cact) ifthe tip shape is known. Contact area determination therefore requiresknowledge of the tip shape.

Three possible approaches to acquiring tip shape are well establishedand practiced either in commercial applications or scientificresearches. A first approach is to directly characterize of tip usingother imaging such as scanning electron microscopy. In this case theoutline of the tip shape is mapped by a fine electron beam with theresolution of a few nanometers (see P. Grutter et al, APPLIED PHYSICSLETTERS 60 (22): 2741-2743 Jun. 1 1992, L. Montelius et al APPLIEDPHYSICS LETTERS 62 (21): 2628-2630 May 24 1993, the subject matter ofwhich is hereby incorporated by reference.) A second approach is toindent the tip on a sample with perfect plastic deformation. In thiscase the plastic deformation of the indent provides a template of thetip shape. A sharper tip or other means of observation such as electronmicroscopy, AFM with a sharper tip are used to create surface image ofthe crater. The same indentation load/displacement curve on a perfectlyplastically deformable sample can also be fitted by so called “areafunction” to give a best guess of the tip shape. Typically, a series ofindents are applied to the reference material over a relatively largerange of maximum loads and maximum penetration depths, hence permittinga measurement of the cross sectional area of the indenter tip as afunction of the distance from the apex. This method has been used byOliver and Pharr (see reference JOURNAL OF MATERIALS RESEARCH 7 (3):613-617 MAR 1992, the subject matter of which is hereby incorporated byreference.)

A third approach uses blind reconstruction of tip topographic imagethrough interacting tip with sharper features and using a morphologicaldilation method to reconstruct the tips shape (Su et al ULTRAMICROSCOPY97 (1-4): 135-144 OCT-NOV 2003; Atamny et al SURFACE SCIENCE 323 (3):L314-L318 JAN 20 1995, the subject matter of which is herebyincorporated by reference.) The advantage of this approach is that thetip shape calibration can be performed in-situ by the AFM and theresolution can be better than the previous two methods. A disadvantageis that the interaction of the tip with sharp feature may bedestructive, and great care need be taken in the imaging process, asdiscussed in the publication.

At the end of these processes, contact stiffness S can be determinedfrom the detected peak pressure P_(max) and the determined penetrationdepth h_(max) as determined by subtracting P_(ic) from P_(max) using avariant equation (7) as derived above:

$\begin{matrix}{S = \frac{L_{m\; {ax}}}{p_{{ma}\; x} - p_{ic}}} & (9)\end{matrix}$

The elastic modulus of the material E_(sample) can then be determinedusing equation as derived above:

E _(sample)=(1−c)/((2√{square root over (A _(com))}/S√{square root over(π)}−(1−c ²)/E _(tip)))  (8)

Creep, a quasistatic measurement, then can made by measuring plasticdeformation for a number of force application rates and by correlatingthose measurements using constitutive equations shown in the referenceof Nowick and Berry (Anelastic Relaxation in Crystalline Solids, thesubject matter of which is hereby incorporated by reference.)Viscoelastic modulus can similarly be determined by measuring thesample's elastic modulus for a number of force application rates and bycorrelating those measurements using the same theory.

A generalized flowchart illustrating a process 330 for obtaining thesemeasurements is illustrated in FIG. 12. Process 330 is identical toprocess 230 discussed above in connection with FIG. 7B but contains anadditional data acquisition loop 356 for controlling the AFM 10 or 110to obtain the data required for mechanical property measurements and toperform those measurements. Process 330 therefore proceeds from Start inBlock 332 to cause the tip to interact with the sample in Block 334,whereupon an indentation control loop 336 and lateral forcecounteraction control loop 338 are performed simultaneously as discussedabove in connection with FIG. 7B. Components of loops 336 and 338 areidentical to the corresponding components of the loops 236 and 238discussed above in connection with FIG. 7B and, accordingly, are denotedby the same reference numerals, incremented by 100.

The data acquisition loop 356 will now be discussed in more detail.

The data acquisition loop 356 begins in Block 358, where an xy positionactuator and/or a z position actuator are controlled and the probe isdriven to oscillate in the manner required to obtain data as discussedabove, e.g., in connection with FIGS. 8-11B. Changes in probeoscillation amplitude, resonant frequency, and/or phase are detected inBlock 360, also as discussed above, to obtain the data required formechanical property measurements. This data may include, for example,P_(ic), P_(r), P_(sep), and P_(max). Then, in Block 362, mechanicalproperty measurements such as plastic deformation, contact stiffness,and elastic modulus are made from the acquired data. Semistaticmeasurements such as creep and visco elastic modulus can be made aftercompletion of a force profile in Block 350.

Although the best mode contemplated by the inventors of carrying out thepresent invention is disclosed above, practice of the present inventionis not limited thereto. It will be manifest that various additions,modifications and rearrangements of the features of the presentinvention may be made without deviating from the spirit and scope of theunderlying inventive concept. The scope of still other changes to thedescribed embodiments that fall within the present invention but thatare not specifically discussed above will become apparent from theappended claims and other attachments.

1. A method comprising: indenting a sample with a probe of a probe-basedinstrument, the probe including a cantilever having a base and a freeend, and the indenting occurring in an indentation cycle having aloading phase in which the probe is driven into the sample to form theindentation and an unloading phase in which the probe is withdrawn fromthe sample, during the indentation cycle, acquiring at least one datumrequired for obtaining a local mechanical property measurement; andusing the acquired datum, obtaining the local mechanical propertymeasurement.
 2. The method of claim 1, wherein the probe is driven tooscillate during at least part of the indentation process, the acquiringstep comprises detecting a change in at least one parameter of probeoscillation resulting from probe/sample interaction during theindentation cycle; and wherein the obtaining step comprises determiningat least one of an initial contact point occurring when the probe firstcontacts the sample during the loading phase and a release pointoccurring when the probe releases from the sample during the unloadingphase.
 3. The method in claim 2, wherein the initial contact point isdetected by detecting a change in at least one of oscillation amplitudeand phase and resonance frequency occurring as a result initialprobe/sample contact.
 4. The method in claim 2, wherein the releasepoint is detected by detecting a change in at least one of probeoscillation amplitude and phase and resonance frequency occurring as aresult of initial tip/sample separation.
 5. The method in claim 2, wherethe datum is obtained by detecting a change in at least one of anoscillation amplitude and phase of sub-resonant oscillation of thecantilever.
 6. The method in claim 2, where the datum is collected bydetecting a change in at least one of an amplitude and a frequency of aprobe oscillating in torsional resonance.
 7. The method of claim 1,wherein the mechanical property includes at least one of elastic modulusand visco-elasticity derived from load/displacement relationship of thecantilever probe at a given contact area.
 8. The method of claim 1,further comprising counteracting lateral forces imposed on the probeduring the indentation cycle using a closed loop feedback process tomaintain a characteristic parameter of the probe a constant.
 9. Themethod of claim 8, wherein the probe includes an active cantilever, andwherein the counteracting step comprises energizing the activecantilever under feedback to impose a force impact on the probe that isof opposite sign to a lateral force on the probe induced by motion ofthe probe upon interacting with the sample.
 10. A method of monitoringprobe/sample interaction during an indentation cycle of a probe-basedinstrument, the indentation cycle including a loading phase in which theprobe is driven into the sample to produce an indentation and anunloading phase in which the probe is withdrawn from the indentation,the method comprising: (A) determining an initial contact pointoccurring when the probe first contacts the sample during the loadingphase, and (B) determining a release point occurring when the probefirst separates from a bottom of the indentation during the unloadingphase of the indentation cycle, the release point being determined bydetecting a change in probe dynamic characteristics resulting frominteraction between the probe and the indentation.
 11. The method ofclaim 10, further comprising determining plastic contact depth bysubtracting the contact point from the release point.
 12. The method ofclaim 10, wherein the initial contact point and release point aredetermined by detecting changes in torsional oscillation characteristicsof the probe, and a relative xy oscillation between the probe and thesample is generated at least in part by shaking the sample in an xyplane.
 13. The method of claim 12, wherein the change in xy oscillationis detected by detecting a change in at least one of a torsionalresonance frequency and a torsional resonance amplitude of the probe.14. The method of claim 10, wherein the detecting step comprisesdetecting the onset of a contact resonance peak occurring when anyportion of the unloading probe separates from the indentation.
 15. Themethod of claim 14, wherein the contact resonance comprises at least oneof torsional resonance and flexural resonance when the probe is incontact with the sample.
 16. The method of claim 10, further comprisingmonitoring changes in at least one of torsional resonance oscillationamplitude and frequency during the unloading phase and determiningcontact area from the resulting resonating probe data.
 17. The method ofclaim 16, wherein the contact area determination relies on the unloadingresonating probe data and characterized probe data.
 18. The method ofclaim 17, further comprising characterizing the probe by determining asurface area of the probe.
 19. The method of claim 18, wherein thecharacterizing step includes indenting a highly plastic referencesample, exciting torsional resonance in the probe at least during theunloading phase of the indentation cycle, and monitoring changes in atleast one of torsional resonance amplitude and phase during theunloading phase of the reference sample indentation cycle.
 20. Themethod of claim 10, further comprising using a closed loop feedbackprocess to counteract lateral forces imposed on the probe during theindentation cycle.
 21. The method of claim 20, wherein the probeincludes an active cantilever that is subject to bending forces uponenergization thereof, and wherein the counteracting step comprisesenergizing at least one of the probe and a z position actuator for theprobe under feedback.
 22. The method of claim 20, further comprisingdetermining a contact depth by subtracting the contact point from therelease point.
 23. The method of claim 10, further comprisingdetermining tip shape through at least one of direct measurement and atip shape reconstruction technique.
 24. A method of monitoring probesample interaction during an indentation cycle of a probe-basedinstrument, the indentation cycle including a loading phase in which theprobe is driven into the sample to produce an indentation and anunloading phase in which the probe is withdrawn from the indentation,the method comprising: (A) driving the probe to oscillate in torsionalresonance; and (B) determining an initial contact point by detecting achange in at least one of torsional resonance frequency and amplitudeoccurring as a result of initial probe/sample contact during the loadingphase.
 25. An instrument comprising: (A) a probe including an activecantilever having a base and a free end; (B) a z position actuator thatdrives at least one of the probe and a sample support to move in a zdirection to alter a probe/sample spacing; and (C) a controller that i.energizes at least one of the active cantilever and the z-positionactuator to effect an indentation cycle including a loading phase inwhich the probe is driven into the sample to produce an indentation andan unloading phase in which the probe is withdrawn from the indentation,ii. determines an initial contact point occurring when the probe firstcontacts the sample during the loading phase, and iii. determines arelease point occurring when the probe first separates from a bottom ofthe indentation during the unloading phase of the indentation cycle, therelease point being determined by detecting a change in relative xyoscillation between the probe and the indentation.
 26. The instrument ofclaim 25, wherein the controller determines a separation point locatedbetween the release point and the sample surface, the separation pointbeing determined by detecting a change in at least one of a torsionalcontact oscillation and a flexural contact oscillation of the probe, andwherein the controller determines contact depth by subtracting theseparation point from the release point.
 27. The instrument of claim 25,wherein the controller acquires data while monitoring changes in atleast one of torsional resonance oscillation amplitude and frequencyduring the unloading phase and determines contact area from the acquireddata.